纺织品中偶氮染料还原液内芳香胺的电喷雾电离质谱分析

在优化的条件下,用电喷雾电离质谱(ESI-MS)检测了多种纺织品中由偶氮染料还原获得的芳香胺。当毛细管温度为100℃、鞘气流速为25单位、进样流速为10μL/min、电压为5kV时,信号的总离子流强度高且较稳定。实验分析了19种致癌芳香胺标准溶液的二级质谱,获得了相应物质的特征碎片离子;在此基础上,建立了基于ESI-MS对毛巾、棉布等样品中芳香胺进行快速定性分析的方法,具有灵敏度高、特异性好、检测速度快等优点。     

火试金法测定铜精矿中金含量结果的不确定度评定

对火试金法测定铜精矿中金含量的结果进行不确定度评定。分析了铜精矿样品称量、铜精矿样品的不均匀性和配料处理,以及金粒称量等因素对金含量测量结果不确定度的影响,并得出火试金法测量铜精矿中金含量的扩展不确定度。     

等离子体质谱法测定玄武岩中微量元素三种样品预处理方法的比较

在测定玄武岩的微量元素时,为了保证得到的微量元素结果反映源区特征,需经预处理去除玄武岩的孔洞中充填的碳酸盐等物质。选取雷州半岛新生代玄武岩三个样品,每一个样品用三种预处理方法进行预处理,等离子体质谱法测定其中的微量元素。分析结果表明,用稀硝酸浸泡样品,会导致玄武岩中大多数微量元素严重丢失,得到的数据失真;而用稀盐酸浸泡去除碳酸盐的方法基本不改变玄武岩中微量元素的含量。     

赣南淘锡坑钨多金属矿床花岗岩和云英岩岩石特征及云英岩中白云母40Ar/39Ar定年

赣南崇义县淘锡坑钨矿位于南岭东西向构造带东段,属于以黑钨矿石英脉型为主的钨多金属矿床。矿床形成与燕山期中酸性岩浆作用有密切关系,石英矿脉受一组北西向断裂控制,穿切新元古界。本文在淘锡坑钨矿区3个揭露到花岗岩体顶部的中段（206、106、56中段）采集到岩体顶部云英岩样品,利用40Ar/39Ar同位素定年测得云英岩中的白云母的坪年龄分别为152.7 ± 1.5 Ma（206中段）,153.4 ± 1.3 Ma（106中段）,155.0 ± 1.4 Ma（56中段）。与前人用其他方法测定的花岗岩成岩和成矿年龄几乎一致。花岗岩和云英岩全岩稀土元素均具有M型四分组效应和强烈的Eu亏损特征,反映出花岗质岩浆经历了高度分异演化及其岩体结晶晚期流体/熔体相互作用。综合前人在南岭地区同类矿床的研究资料,可知南岭地区160～150Ma成岩成矿作用主要分布于南岭中-东段,可能为大陆边缘弧后岩石圈伸展的构造动力学背景的产物。     

Zircon U–Pb ages, Hf and O isotopes constrain the crustal architecture of the ultrahigh-pressure Dabie orogen in China

The crustal structure of the Dabie orogen was reconstructed by a combined study of U–Pb ages, Hf and O isotope compositions of zircons from granitic gneiss from North Dabie, the largest lithotectonic unit in the orogen. The results were deciphered from metamorphic history to protolith origin with respect to continental subduction and exhumation. Zircon U–Pb dating provides consistent ages of 751 ± 7 Ma for protolith crystallization, and two group ages of 213 ± 4 to 245 ± 17 Ma and 126 ± 4 to 131 ± 36 Ma for regional metamorphism. Majority of zircon Hf isotope analyses displays negative ε_Hf(t) values of − 5.1 to − 2.9 with crust Hf model ages of 1.84 to 1.99 Ga, indicating protolith origin from reworking of middle Paleoproterozoic crust. The remaining analyses exhibit positive ε_Hf(t) values of 5.3 to 14.5 with mantle Hf model ages of 0.74 to 1.11 Ga, suggesting prompt reworking of Late Mesoproterozoic to Early Neoproterozoic juvenile crust. Zircon O isotope analyses yield δ¹⁸O values of − 3.26 to 2.79‰, indicating differential involvement of meteoric water in protolith magma by remelting of hydrothermally altered low δ¹⁸O rocks. North Dabie shares the same age of Neoproterozoic low δ¹⁸O protolith with Central Dabie experiencing the Triassic UHP metamorphism, but it was significantly reworked at Early Cretaceous in association with contemporaneous magma emplacement. The Rodinia breakup at about 750 Ma would lead to not only the reworking of juvenile crust in an active rift zone for bimodal protolith of Central Dabie, but also reworking of ancient crust in an arc-continent collision zone for the North Dabie protolith. The spatial difference in the metamorphic age (Triassic vs. Cretaceous) between the northern and southern parts of North Dabie suggests intra-crustal detachment during the continental subduction. Furthermore, the Dabie orogen would have a three-layer structure prior to the Early Cretaceous magmatism: Central Dabie in the upper, North Dabie in the middle, and the source region of Cretaceous magmas in the lower.     

Dehydration and melting during continental collision: Constraints from element and isotope geochemistry of low-T/UHP granitic gneiss in the Dabie orogen

A combined study of petrography, whole-rock major and trace elements as well as Rb?Sr and Sm?Nd isotopes, and mineral oxygen isotopes was carried out for two groups of low-T/UHP granitic gneiss in the Dabie orogen. The results demonstrate that metamorphic dehydration and partial melting occurred during exhumation of deeply subducted continent. Zircon δ¹⁸O values of ? 2.8 to + 4.7‰ for the gneiss are all lower than normal mantle values of 5.3 ± 0.3‰, consistent with ¹⁸O depletion of protolith due to high-T meteoric-hydrothermal alteration at mid-Neoproterozoic. Most samples have extremely low ⁸⁷Sr/⁸⁶Sr ratios at t₁ = 780 Ma, but very high ⁸⁷Sr/⁸⁶Sr ratios at t₂ = 230 Ma. This suggests intensive fluid disturbance due to the hydrothermal alteration of protoliths during Neoproterozoic magma emplacement and the metamorphic dehydration during Triassic continental collision. Rb–Sr isotopes, Th/Ta vs. La/Ta and Th/Hf vs. La/Nb relationships suggest that Group I gneiss experienced lower degrees of hydrothermal alteration, but higher degrees of dehydration, than Group II gneiss. The two groups of gneiss have similar patterns of REE and trace element partition. Group I gneiss displays good correlations between Nb and LREEs but no correlations between Nb and LILEs (Rb, Ba, Pb, Th and U), indicating differential mobilities of LILEs during the dehydration. Thus the correlation between Nb and LREEs is inherited from protolith rather than caused by metamorphic modification. Relative to Group I gneiss, Group II gneiss has stronger negative Eu anomaly, lower contents of Sr and Ba but higher contents of Rb, Th and U. In particular, Nb correlates with LILEs (e.g., Rb, Sr, Ba, Th and U), but not with LREEs (La and Ce). This may indicate decoupling between the dehydration and LILEs transport during continental collision. Furthermore, dehydration melting may have occurred due to breakdown of muscovite during “hot” exhumation. Group II gneiss has extremely low contents of FeO + MgO + TiO₂ (1.04 to 2.08 wt.%), high SiO₂ contents of 75.33 to 78.23 wt%, and high total alkali (Na₂O + K₂O) contents (7.52 to 8.92 wt.%), comparable with compositions predicted from partial melting of felsic rocks by experimental studies. Almost no UHP metamorphic minerals survived; felsic veins of fine-grain minerals occurs locally between coarse-grain minerals, resulting in a kind of metatexite migmatites due to dehydration melting without considerable escape of felsic melts from the host gneiss. In contrast, Group I gneiss only shows metamorphic dehydration. Therefore, the two groups of gneiss show contrasting behaviors of fluid–rock interaction during the continental collision.     

Comparison of arsenic concentrations in simultaneously-collected groundwater and aquifer particles from Bangladesh,India, Vietnam,and Nepal

One of the reasons the processes resulting in As release to groundwater in southern Asia remain poorly understood is the high degree of spatial variability of physical and chemical properties in shallow aquifers. In an attempt to overcome this difficulty, a simple device that collects groundwater and sediment as a slurry from precisely the same interval was developed in Bangladesh. Recently published results from Bangladesh and India relying on the needle-sampler are augmented here with new data from 37 intervals of grey aquifer material of likely Holocene age in Vietnam and Nepal. A total of 145 samples of filtered groundwater ranging in depth from 3 to 36 m that were analyzed for As (1–1000 μg/L), Fe (0.01–40 mg/L), Mn (0.2–4 mg/L) and S (0.04–14 mg/L) are compared. The P-extractable (0.01–36 mg/kg) and HCl-extractable As (0.04–36 mg/kg) content of the particulate phase was determined in the same suite of samples, in addition to Fe(II)/Fe ratios (0.2–1.0) in the acid-leachable fraction of the particulate phase. Needle-sampler data from Bangladesh indicated a relationship between dissolved As in groundwater and P-extractable As in the particulate phase that was interpreted as an indication of adsorptive equilibrium, under sufficiently reducing conditions, across 3 orders of magnitude in concentrations according to a distribution coefficient of 4 mL/g. The more recent observations from India, Vietnam and Nepal show groundwater As concentrations that are often an order of magnitude lower at a given level of P-extractable As compared to Bangladesh, even if only the subset of particularly reducing intervals characterized by leachable Fe(II)/Fe >0.5 and dissolved Fe >0.2 mg/L are considered. Without attempting to explain why As appears to be particularly mobile in reducing aquifers of Bangladesh compared to the other regions, the consequences of increasing the distribution coefficient for As between the particulate and dissolved phase to 40 mL/g for the flushing of shallow aquifers of their initial As content are explored.     

Considerations for conducting incubations to study the mechanisms of As release in reducing groundwater aquifers

Microbial Fe reduction is widely believed to be the primary mechanism of As release from aquifer sands in Bangladesh, but alternative explanations have been proposed. Long-term incubation studies using natural aquifer material are one way to address such divergent views. This study addresses two issues related to this approach: (1) the need for suitable abiotic controls and (2) the spatial variability of the composition of aquifer sands. Four sterilization techniques were examined using orange-colored Pleistocene sediment from Bangladesh and artificial groundwater over 8 months. Acetate (10 mM) was added to sacrificial vials before sterilization using either (1) 25 kGy of gamma irradiation, (2) three 1-h autoclave cycles, (3) a single addition of an antibiotic mixture at 1× or (4) 10× the typical dose, and (5) a 10 mM addition of azide. The effectiveness of sterilization was evaluated using two indicators of microbial Fe reduction, changes in diffuse spectral reflectance and leachable Fe(II)/Fe ratios, as well as changes in P-extractable As concentrations in the solid phase. A low dose of antibiotics was ineffective after 70 days, whereas autoclaving significantly altered groundwater composition. Gamma irradiation, a high dose of antibiotics, and azide were effective for the duration of the experiment.